Device for generating oxygen

ABSTRACT

A device for generating oxygen comprising at least one reaction chamber for housing a composition for generating oxygen, the composition comprising a combination of constituents consisting of at least one oxygen source, at least one ionic liquid, and at least one metal oxide compound, means for maintaining at least one of the oxygen source, the ionic liquid and the metal oxide compound physically separated from the remaining constituents, means for establishing physical contact of the oxygen source, the ionic liquid and the metal oxide compound, and means for allowing oxygen to exit the reaction chamber, wherein the metal oxide compound is an oxide of a single metal or of two or more different metals, said metal(s) being selected from the metals of groups 2 to 14 of the periodic table of the elements, and wherein the oxygen source comprises a peroxide compound.

FOREIGN PRIORITY

This application claims priority to European Patent Application No.16199637.6 filed Nov. 18, 2016, the entire contents of which isincorporated herein by reference.

TECHNICAL FIELD

The present invention relates to devices for generating oxygen.

BACKGROUND

Humans cannot exist without oxygen. In many environments, however,oxygen supply is insufficient or there is a risk of emergency situationsinvolving a shortage of oxygen, for example in submarines, in mines, inspace capsules, and also in air planes. Air pressure decreases withincreasing flight altitude, and at cruising altitudes of many aircrafts,in particular long-range aircrafts, sufficient oxygen for human beingsis no longer available. Therefore, the aircraft cabins are pressurizedin order to ensure sufficient oxygen supply. In case of a suddendepressurization of an aircraft cabin, oxygen masks must be available,which supply oxygen to crew and passengers until the aircraft reaches aflight level where sufficient oxygen is available.

The oxygen which is provided by these emergency systems is typicallyproduced by so-called “chlorate candles” or “oxygen candles”. Thesechemical oxygen generators contain chlorates or perchlorates as anoxygen source, as well as various additives such as fuels, catalysts,binders and moderators. Chlorate candles are often in the form ofcylindrical rods, i.e. they have a shape similar to candles. Chloratecandles are disclosed, for example, in WO 97/43210.

Known chlorate candles require high temperatures at which the oxygenproduction takes place. Namely, in chlorate candles oxygen is releasedat temperatures between 450° C. and 700° C. Therefore, effective heatinsulation of chlorate candles is required, resulting in a weight andsize penalty. Furthermore, decomposition of chlorates and perchloratestends to produce toxic side products, in particular chlorine, which mustbe removed from the oxygen stream, thus additionally adding size andweight. Furthermore, there is a risk of system failure. In chloratecandles the reaction zone is normally liquid, i.e. there is a liquidzone travelling through the candle, starting at the point of ignition.The liquid zone within the otherwise solid candle considerablydestabilizes the candle such that mechanical shocks or even slightvibrations may result in separation of the candle portions, thusinterrupting the heat transfer and discontinuing the chlorate orperchlorate decomposition. In such a case, oxygen production may beinterrupted, although oxygen is still vitally needed.

A different type of chemical oxygen generators uses peroxides as oxygensources, for example sodium percarbonate, sodium perborate, or a ureaadduct of hydrogen peroxide. Decomposition of the peroxides yieldsoxygen, and the decomposition reaction can be started by contacting theperoxide compounds with an appropriate enzyme or transition metalcatalyst. Chemical oxygen generators of this type are disclosed in U.S.Pat. No. 2,035,896, WO 86/02063, JPS 61227903, and DE 196 02 149.

Many known peroxide-based oxygen generators use water for providingcontact between the peroxides and the catalysts. Unfortunately, waterfreezes at 0° C. and, therefore, no oxygen can be produced below 0° C.,while some emergency systems must be operational below 0° C. Also, thedecomposition of peroxides in aqueous solutions may result in vehementeffervescing of the reaction mixture. As a consequence, an oxygengenerating device containing a peroxide-based oxygen generatingcomposition must have a complicated structure.

It would be beneficial to provide a solution to at least some of theproblems of the prior art outlined above, and to provide a device forgenerating oxygen capable of producing breathable oxygen reliably andcontinuously in a wide temperature range, and preferably includingsubfreezing temperatures. The oxygen produced should be at a lowtemperature, preferably below 150° C., and further preferably free fromtoxic or otherwise noxious components such as chlorine or carbonmonoxide. It would be also beneficial to provide a device capable toproduce oxygen over an extended period of time and with a significantflow rate. It would be further beneficial to provide a device forgenerating oxygen, the device having minimum space requirements andbeing lightweight and simple in structure.

SUMMARY

Exemplary embodiments of the invention include A device for generatingoxygen comprising at least one reaction chamber for housing acomposition for generating oxygen, the composition comprising acombination of constituents consisting of at least one oxygen source, atleast one ionic liquid, and at least one metal oxide compound, means formaintaining at least one of the oxygen source, the ionic liquid and themetal oxide compound physically separated from the remainingconstituents, means for establishing physical contact of the oxygensource, the ionic liquid and the metal oxide compound, and means forallowing oxygen to exit the reaction chamber, wherein the metal oxidecompound is an oxide of a single metal or of two or more differentmetals, said metal(s) being selected from the metals of groups 2 to 14of the periodic table of the elements, and wherein the oxygen sourcecomprises a peroxide compound.

Exemplary embodiments of the invention also include a charge componentfor a device for generating oxygen, the charge component comprising anoxygen source formulation and/or an ionic liquid formulation and/or ametal oxide compound formulation, wherein the oxygen source formulationcomprises a peroxide compound, the ionic liquid formulation is in theliquid state at least in a temperature range from −10° C. to +50° C.,and the metal oxide compound formulation comprises an oxide of onesingle metal or of two or more different metals, said metal(s) beingselected from the metals of groups 2 to 14 of the periodic table of theelements.

Exemplary embodiments of the invention are based on an entirely newconcept, the use of ionic liquids in chemical oxygen generatingcompositions.

Technical implementations of this inventive concept include acomposition for generating oxygen, a method for generating oxygen fromthis composition, a device for generating oxygen containing thecomposition, and the use of an ionic liquid as a dispersant or solventand/or as a heat sink in the composition and/or for releasing oxygenfrom the composition over an extended period of time.

Implementations of this inventive concept also include the compositionbeing in the form of a kit, i.e. in a form preventing that allconstituents of the composition, which are required for initiating andsupporting oxygen generation, can come into physical contact with eachother.

Implementations of this invention further include that the kit isspecifically adapted for filling or refilling a device for generatingoxygen according to this invention.

As can be easily understood, the constituents of the composition are thesame, irrespective of which technical implementation of the invention iscontemplated. Therefore, any disclosure provided for a particularimplementation, such as composition, device, method or use, isanalogously applicable to the other implementations of this invention.

Embodiments 1 to 83 below constitute exemplary implementations of thisinvention.

1. A composition for generating oxygen, comprising

-   -   at least one oxygen source,    -   at least one ionic liquid, and    -   at least one metal oxide compound, wherein        -   the oxygen source comprises a peroxide compound,        -   the ionic liquid is in the liquid state at least in a            temperature range from −10° C. to +50° C., and        -   the metal oxide compound is an oxide of one single metal or            of two or more different metals, said metal(s) being            selected from the metals of groups 2 to 14 of the periodic            table of the elements.

2. The composition according to embodiment 1, wherein the oxygen sourceand the metal oxide compound, or the oxygen source and the ionic liquid,or the metal oxide compound and the ionic liquid, are not in physicalcontact with each other.

3. The composition according to embodiment 1 or 2, wherein the oxygensource is selected from alkali metal percarbonates, alkali metalperborates, urea hydrogen peroxide, and mixtures thereof.

4. The composition according to any one of embodiments 1 to 3, whereinthe oxygen source is one or more of Na2CO3×1.5 H202, NaBO3×4H2O,NaBO3×H2O and urea hydrogen peroxide.

5. The composition according to any one of embodiments 1 to 4, whereinthe ionic liquid is at least one salt having a cation and an anion,wherein the cation is selected from the group consisting of imidazolium,pyrrolidinium, ammonium, choline, pyridinium, pyrazolium, piperidinium,phosphonium, and sulfonium cations, and wherein the cation may have atleast one substituent.

6. The composition according to any one of embodiments 1 to 5, whereinthe ionic liquid is at least one salt having a cation and an anion,wherein the anion is selected from the group consisting ofdimethylphosphate, methylsulfate, trifluoromethylsulfonate,bis(trifluoromethylsulfonyl)imide, chloride, bromide, iodide,tetrafluoroborate, and hexafluorophosphate.

7. The composition according to any one of embodiments 1 to 6, whereinthe ionic liquid is selected from the group consisting of

-   -   butyltrimethylammoniumbis(trifluoromethylsulfonyl)imide        ([Me3BuN]TFSI)    -   1-butyl-3-methylimidazoliumtrifluoromethanesulfonate (BMImOTf),    -   1-butyl-3-methylimidazoliumdimethylphosphate (BMImPO₄Me₂),    -   1-butyl-3-methylimidazoliummethylsulfate (BMImSO₄Me),    -   1,1-butylmethylpyrrolidiniumbis(trifluoromethylsulfonyl)imide        (BmpyrTFSI),    -   1,3-dimethylimidazoliumdimethylphosphate (MMImPO₄Me₂),    -   1,3-dimethylimidazoliummethylsulfate (MMImSO₄Me).

8. The composition according to any one of embodiments 1 to 7, whereinthe metal oxide compound is at least one oxide containing one singlemetal, optionally in different oxidation states.

9. The composition according to any one of embodiments 1 to 8, whereinthe metal oxide compound is one or more of MnO2, Co3O4, CrO3, Ag2O, CuO,and PbO2.

10. The composition according to any one of embodiments 1 to 9, whereinthe metal oxide compound is at least one oxide containing at least twodifferent metals.

11. The composition according to anyone of embodiments 1 to 10, whereinthe metal oxide compound is selected from spinel type metal oxides,ilmenite type metal oxides and perovskite type metal oxides.

12. The composition according to anyone of embodiments 1 to 11, whereinthe metal oxide compound is selected from mixed cobalt iron oxides,mixed copper iron oxides, mixed nickel iron oxides, mixed manganese ironoxides, mixed copper manganese oxides, mixed cobalt manganese oxides,mixed nickel manganese oxides, mixed nickel cobalt oxides, mixedlanthanum iron nickel oxides, mixed lanthanum strontium manganese oxide,and mixtures thereof.

13. The composition according to any one of embodiments 1 to 12, whereinthe metal oxide compound is at least one of CoFe2O4, Co1.5Fe1.5O4,Co2FeO4, CuFe2O4, Cu1.5Mn1.5O4, Co2MnO4, NiMnO3, NiCo2O4,La0.5Sr0.5MnO3, and LaFe0.25Ni0.7503.

14. The composition according to any one of embodiments 1 to 13, whereinthe composition is provided as a kit of at least two physicallyseparated components, each component lacking at least one of the oxygensource, the ionic liquid, and the metal oxide compound.

15. The composition according to embodiment 14, wherein one componentcomprises a metal oxide compound formulation and the ionic liquidformulation, and the other component comprises an oxygen sourceformulation.

16. The composition according to embodiment 14, wherein one componentcomprises an oxygen source formulation and a metal oxide compoundformulation, and the other component comprises a ionic liquidformulation.

17. The composition according to embodiment 14, wherein the kitcomprises a third component, one component comprising an oxygen sourceformulation, the other component comprising a ionic liquid formulation,and the third component comprising a metal oxide compound formulation.

18. The composition according to any one of embodiments 1 to 17, whereinthe oxygen source is present in an amount ranging from 10 to 80 weight %of the composition, the ionic liquid is present in an amount rangingfrom 20 to 80 weight % of the composition, and the metal oxide compoundis present in an amount ranging from more than 0 to 20 weight % of thecomposition.

19. The composition according to any one of embodiments 1 to 18, whereinat least one of the oxygen source and the metal oxide compound is in theform of powders or is in the form of at least one powder compact.

20. The composition according to embodiment 19, wherein the at least onepowder compact has been compacted with a pressure in the range of 1 to220 MPa.

21. The composition according to any one of embodiments 14 to 20,wherein the kit comprises at least two different metal oxide compoundsand/or at least two peroxide compound which differ in degree ofcompaction.

22. A method for generating oxygen comprising

-   -   providing at least one oxygen source,    -   providing at least one ionic liquid,    -   providing at least one metal oxide compound, wherein        -   the oxygen source is a peroxide compound,        -   the ionic liquid is in the liquid state at least in the            temperature range from −10° C. to +50° C., and        -   the metal oxide compound is an oxide of one single metal or            of two or more different metals, said metal(s) being            selected from the metals of groups 2 to 14 of the periodic            table of the elements, and    -   contacting the oxygen source, the ionic liquid, and the metal        oxide compound.

23. The method according to embodiment 22, wherein the oxygen source andthe ionic liquid are provided as a first component, the metal oxidecompound is provided as a second component, and the step of contactingcomprises mixing the first and the second components.

24. The method according to embodiment 22, wherein the metal oxidecompound and the ionic liquid are provided as a first component, theoxygen source is provided as a second component, and the step ofcontacting comprises mixing the first and the second component.

25. The method according to embodiment 22, wherein the oxygen source andthe metal oxide compound are provided as a first component, the ionicliquid is provided as a second component, and the step of contactingcomprises mixing the first and the second components.

26. The method according to embodiment 22, wherein the oxygen source isprovided as a first component, the ionic liquid is provided as a secondcomponent, the metal oxide compound is provided as a third component,and the step of contacting comprises mixing the first, the second, andthe third components.

27. The method according to any one of embodiments 22 to 26, wherein theoxygen source is selected from alkali metal percarbonates, alkali metalperborates, urea hydrogen peroxide, and mixtures thereof.

28. The method according to any one of embodiments 22 to 27, wherein theoxygen source is one or more of Na2CO3×1.5 H2O2, NaBO3×4H2O, NaBO3×H2O,and urea hydrogen peroxide.

29. The method according to any one of embodiments 22 to 28, wherein theionic liquid is at least one salt having a cation and an anion, whereinthe cation is selected from the group consisting of imidazolium,pyrrolidinium, ammonium, choline, pyridinium, pyrazolium, piperidinium,phosphonium, and sulfonium cations, and wherein the cation may have atleast one substituent.

30. The method according to any one of embodiments 22 to 29, wherein theionic liquid is at least one salt having a cation and an anion, whereinthe anion is selected from the group consisting of dimethylphosphate,methylsulfate, trifluoromethylsulfonate,bis(trifluoromethylsulfonyl)imide, chloride, bromide, iodide,tetrafluoroborate, and hexafluorophosphate.

31. The method according to any one of embodiments 22 to 30, wherein theionic liquid is selected from the group consisting of

-   butyltrimethylammoniumbis(trifluoromethylsulfonyl)imide    ([Me3BuN]TFSI)-   1-butyl-3-methylimidazoliumtrifluoromethanesulfonate (BMImOTf),-   1-butyl-3-methylimidazoliumdimethylphosphate (BMImPO₄Me₂),-   1-butyl-3-methylimidazoliummethylsulfate (BMImSO₄Me),-   1,1-butylmethylpyrrolidiniumbis(trifluoromethylsulfon)imide    (BmpyrTFSI),-   1,3-dimethylimidazoliumdimethylphosphate (MMImPO₄Me₂),-   1,3-dimethylimidazoliummethylsulfate (MMImSO₄Me).

32. The method according to any one of embodiments 22 to 31, wherein themetal oxide compound is at least one oxide containing one single metal,optionally in different oxidation states.

33. The method according to any one of embodiments 22 to 32, wherein themetal oxide compound is one or more of MnO2, Co3O4, CrO3, Ag2O, CuO, andPbO2.

34. The method according to any one of embodiments 22 to 33, wherein themetal oxide compound is at least on oxide containing at least twodifferent metals.

35. The method according to any one of embodiments 22 to 34, wherein themetal oxide compound is selected from spinel type metal oxides, ilmenitetype metal oxides and perovskite type metal oxides.

36. The method according to any one of embodiments 22 to 35, wherein themetal oxide compound is selected from mixed cobalt iron oxides, mixedcopper iron oxides, mixed nickel iron oxides, mixed manganese ironoxides, mixed copper manganese oxides, mixed cobalt manganese oxides,mixed nickel manganese oxides, mixed nickel cobalt oxides, mixedlanthanum iron nickel oxides, mixed lanthanum strontium manganese oxide,and mixtures thereof.

37. The method composition according to any one of embodiments 22 to 36,wherein the metal oxide compound is at least one of CoFe204,Co1.5Fe1.5O4, Co2FeO4, CuFe2O4, Cu1.5Mn1.5O4, Co2MnO4, NiMnO3, Ni-Co2O4,La0.5Sr0.5MnO3, and LaFe0.25Ni0.75O3.

38. The method according to any one of embodiments 22 to 37, wherein atleast one of the oxygen source and the metal oxide compound is in theform of powder.

39. The method according to any one of embodiments 22 to 38, wherein atleast one of the oxygen source and the metal oxide compound is in theform of at least one powder compact.

40. The method according to embodiment 39, wherein the at least onepowder compact has been compacted with a pressure in the range of 1 to220 MPa.

41. The method according to embodiment 39 or 40, wherein at least one ofthe oxygen source and the metal oxide compound includes powder compactshaving different degrees of compression.

42. The method according to any one of embodiments 22 to 41, wherein theoxygen source and the metal oxide compound are provided as a mixture.

43. The method according to any one of embodiments 22 to 42, wherein theoxygen source is present in an amount ranging from 10 to 80 weight % ofthe composition, the ionic liquid is present in an amount ranging from20 to 80 weight % of the composition, and the metal oxide compound ispresent in an amount ranging from more than 0 to 20 weight % of thecomposition.

44. A device for generating oxygen comprising

-   -   at least one reaction chamber for housing a composition for        generating oxygen, the composition comprising a combination of        constituents consisting of at least one oxygen source, at least        one ionic liquid, and at least one metal oxide compound,        -   means for maintaining at least one of the oxygen source, the            ionic liquid and the metal oxide compound physically            separated from the remaining constituents,        -   means for establishing physical contact of the oxygen            source, the ionic liquid and the metal oxide compound, and        -   means for allowing oxygen to exit the reaction chamber,    -   wherein the metal oxide compound is an oxide of a single metal        or of two or more different metals, said metal(s) being selected        from the metals of groups 2 to 14 of the periodic table of the        elements, and wherein the oxygen source comprises a peroxide        compound.

45. The device according to embodiment 44, wherein the means forallowing oxygen to exit the reaction chamber is selected from a gaspermeable membrane, a frit and a molecular sieve.

46. The device according to embodiment 44 or 45, wherein the reactionchamber comprises a first compartment for receiving at least one of theoxygen source, the ionic liquid and the metal oxide compound, and asecond compartment for receiving the other constituents.

47. The device according to any one of embodiments 44 to 46, wherein themeans for maintaining at least one of the oxygen source, the ionicliquid and the metal oxide compound physically separated comprise atleast one receptacle within the chamber for receiving at least one ofthe oxygen source, the ionic liquid and the metal oxide compound.

48. The device according to any one of embodiments 44 to 47, wherein themeans for maintaining at least one of the oxygen source, the ionicliquid and the metal oxide compound physically separated comprise amembrane, a foil, or a glass plate between the first compartment and thesecond compartment.

49. The device according to any one of embodiments 44 to 48, wherein themeans for establishing physical contact comprise a device for destroyingthe means for maintaining the constituents physically separated, and anactivation mechanism for activating the device.

50. The device according to any one of embodiments 44 to 49, wherein thedevice for destroying is a solid plate, a grid, or a cutting edge.

51. The device according to any one of embodiments 44 to 50, wherein themeans for establishing physical contact is a syringe or a dosingmechanism.

52. The device according to any one of embodiments 44 to 51, wherein theat least one reaction chamber is placed within a container having a gasoutlet.

53. The device according to any one of embodiments 44 to 52, wherein atleast two reaction chambers are placed within a container, the containerproviding a common gas space for receiving oxygen exiting the reactionchambers.

54. The device according to any one of embodiments 44 to 53, whereinfrom three to 20 reaction chambers are placed within a container, thecontainer providing a common gas space for receiving oxygen exiting thereaction chambers.

55. The device according to any one of embodiments 44 to 54, wherein theat least one reaction chamber comprises different compositions forgenerating oxygen.

56. The device according to embodiment 53, wherein at least two reactionchambers comprise different compositions for generating oxygen.

57. The device according to any one of embodiments 52 to 56, wherein thegas outlet comprises means for restricting gas flow.

58. The device according to any one of embodiments 55 to 57, wherein thecompositions for generating oxygen differ with respect to the oxygensource and/or with respect to the ionic liquid and/or with respect tothe metal oxide compound and/or with respect to degree of compaction ofthe oxygen source.

59. A charge component for a device for generating oxygen as embodied inany one of embodiments 44 to 58, the charge component comprising anoxygen source formulation and/or an ionic liquid formulation and/or ametal oxide compound formulation, wherein

-   -   the oxygen source formulation comprises a peroxide compound,    -   the ionic liquid formulation is in the liquid state at least in        a temperature range from −10° C. to +50° C., and    -   the metal oxide compound formulation comprises an oxide of one        single metal or of two or more different metals, said metal(s)        being selected from the metals of groups 2 to 14 of the periodic        table of the elements.

60. The charge component according to embodiment 59, wherein theperoxide compound is selected from alkali metal percarbonates, alkalimetal perborates, urea hydrogen peroxide, and mixtures thereof.

61. The charge component according to embodiment 59 or 60, wherein theionic liquid formulation comprises an ionic liquid having a cation andan anion, wherein the cation is selected from the group consisting ofimidazolium, pyrrolidinium, ammonium, choline, pyridinium, pyrazolium,piperidinium, phosphonium, and sulfonium cations, and wherein the cationmay have at least one substituent, and wherein the anion is selectedfrom the group consisting of dimethylphosphate, methylsulfate,trifluoromethylsulfonate, bis(trifluoromethylsulfonyl)imide, chloride,bromide, iodide, tetrafluoroborate, and hexafluorophosphate.

62. The charge component according to any one of embodiments 59 to 61,wherein the metal oxide compound is one or more of MnO2, Co3O4, CrO3,Ag2O, CuO, and PbO2.

63. The charge component according to any one of embodiments 59 to 62,wherein the metal oxide compound is selected from spinel type metaloxides, ilmenite type metal oxides and perovskite type metal oxides.

64. The charge component according to any one of embodiments 59 to 63,wherein the metal oxide compound is selected from mixed cobalt ironoxides, mixed copper iron oxides, mixed nickel iron oxides, mixedmanganese iron oxides, mixed copper manganese oxides, mixed cobaltmanganese oxides, mixed nickel manganese oxides, mixed nickel cobaltoxides, and mixed lanthanum iron nickel oxides, mixed lanthanumstrontium manganese oxide, and mixtures thereof.

65. The charge component according to any one of embodiments 59 to 64,wherein at least one of the oxygen source formulation and the metaloxide compound formulation is in the form of powders or is in the formof at least one powder compact.

66. Use of an ionic liquid as a dispersant or solvent and as a heat sinkin a composition for generating oxygen, the composition furthercomprising

-   -   at least one oxygen source formulation, and    -   at least one metal oxide compound formulation, wherein    -   the oxygen source formulation comprises a peroxide compound,    -   the ionic liquid is in the liquid state at least in a        temperature range from −10° C. to +50° C., and    -   the metal oxide compound formulation comprises a metal oxide        compound which is an oxide of one single metal or of two or more        different metals, said metal(s) being selected from the metals        of groups 2 to 14 of the periodic table of the elements.

67. The use according to embodiment 66, wherein the peroxide compound isselected from alkali metal percarbonates, alkali metal perborates, ureahydrogen peroxide, and mixtures thereof.

68. The use according to embodiment 66 or 67, wherein the peroxidecompound is one or more of Na2CO3×1.5 H2O2, NaBO3×4H2O, NaBO3×H2O, andurea hydrogen peroxide.

69. The use according to any one of embodiments 66 to 68, wherein theionic liquid is at least one salt having a cation and an anion, whereinthe cation is selected from the group consisting of imidazolium,pyrrolidinium, ammonium, choline, pyridinium, pyrazolium, piperidinium,phosphonium, and sulfonium cations, and wherein the cation may have atleast one substituent.

70. The use according to any one of embodiments 66 to 69, wherein theionic liquid is at least one salt having a cation and an anion, whereinthe anion is selected from the group consisting of dimethylphosphate,methylsulfate, trifluoromethylsulfonate,bis(trifluoromethylsulfonyl)imide, chloride, bromide, iodide,tetrafluoroborate, and hexafluorophosphate.

71. The use according to any one of embodiments 66 to 70, wherein theionic liquid is selected from the group consisting of

-   butyltrimethylammoniumbis(trifluoromethylsulfonyl)imide    ([Me3BuN]TFSI)-   1-butyl-3-methylimidazoliumtrifluoromethanesulfonate (BMImOTf),-   1-butyl-3-methylimidazoliumdimethylphosphate (BMImPO₄Me₂),-   1-butyl-3-methylimidazoliummethylsulfate (BMImSO₄Me),-   1,1-butylmethylpyrrolidiniumbis(trifluoromethylsulfonyl)imide    (BmpyrTFSI),-   1,3-dimethylimidazoliumdimethylphosphate (MMImPO₄Me₂),-   1,3-dimethylimidazoliummethylsulfate (MMImSO₄Me).

72. The use according to any one of embodiments 66 to 71, wherein themetal oxide compound is at least one oxide containing one single metal,optionally in different oxidation states.

73. The use according to any one of embodiments 66 to 72, wherein themetal oxide compound is one or more of MnO2, Co3O4, CrO3, Ag2O, CuO, andPbO2.

74. The use according to any one of embodiments 66 to 73, wherein themetal oxide compound is at least one oxide containing at least twodifferent metals.

75. The use according to any one of embodiments 66 to 74, wherein themetal oxide compound is selected from spinel type metal oxides, ilmenitetype metal oxides and perovskite type metal oxides.

76. The use according to any one of embodiments 66 to 75, wherein themetal oxide compound is selected from mixed cobalt iron oxides, mixedcopper iron oxides, mixed nickel iron oxides, mixed manganese ironoxides, mixed copper manganese oxides, mixed cobalt manganese oxides,mixed nickel manganese oxides, mixed nickel cobalt oxides, mixedlanthanum iron nickel oxides, mixed lanthanum strontium manganese oxideand mixtures thereof.

77. The use according to any one of embodiments 66 to 76, wherein themetal oxide compound is at least one of CoFe2O4, Co1.5Fe1.5O4, Co2FeO4,CuFe2O4, Cu1.5Mn1.5O4, Co2MnO4, NiMnO3, NiCo2O4, and La0.5Sr0.5MnO3.

78. The use according to any one of embodiments 66 to 77, wherein theoxygen source is present in an amount ranging from 10 to 80 weight % ofthe composition, the ionic liquid is present in an amount ranging from20 to 80 weight % of the composition, and the metal oxide compound ispresent in an amount ranging from more than 0 to 20 weight % of thecomposition.

79. The use according to any one of embodiments 66 to 78, wherein atleast one of the oxygen source formulation and the metal oxide compoundformulation is in the form of powders or is in the form of at least onepowder compact.

80. The use according to embodiment 79, wherein the at least one powdercompact has been compacted with a pressure in the range of 1 to 220 MPa.

81. The use according to embodiment 79 or 80, wherein the oxygen sourceformulation comprises at least two different peroxide compounds and/orat least two peroxide compounds which differ in degree of compaction.

82. The use according to any one of embodiments 79 to 81, wherein themetal oxide compound formulation comprises at least two different metaloxide compounds and/or at least two metal oxide compounds which differin degree of compaction.

83. Use of an ionic liquid for releasing oxygen from a composition forgenerating oxygen over an extended period of time, the composition forgenerating oxygen having the features as defined in any one ofembodiments 66 to 82.

A composition, method, device or use for generating oxygen in the senseof this invention is a composition, method, device or use intended forgenerating oxygen, while any composition, method, device or use whichmay generate oxygen as a side reaction does not constitute acomposition, method, device or use in the sense of this invention.

The oxygen generating compositions according to exemplary embodiments ofthe invention comprise, as the essential constituents, at least oneperoxide compound as an oxygen source, at least one metal oxide compoundas a catalyst triggering the oxygen release reaction, and at least oneionic liquid as a carrier for providing contact between the oxygensource and the catalyst, and for dissipating the heat generated duringthe peroxide decomposition reaction.

The present inventors found that peroxide compounds such as hydrogenperoxide adduct compounds, can be decomposed in ionic liquids bycontacting them with metal oxides in a similar manner as in aqueoussolution, but without the disadvantages of aqueous solutions. Exemplarycomposition of this invention do not contain any water. In particular,decomposition of peroxide compounds in ionic liquids yields breathableoxygen at low temperatures, and without requiring bulky thermalinsulations for the oxygen generating device.

This can be attributed to the use of ionic liquids as a medium forproviding contact between the oxygen source and the catalyst.

Ionic liquids are salts in the liquid state. Therefore, any salt thatmelts without decomposing or vaporizing yields an ionic liquid.Sometimes, salts which are liquid below the boiling point of water areconsidered as ionic liquids. Technically interesting are in particularthose ionic liquids which are in the liquid state at relatively lowtemperatures such as at room temperature or even below room temperature.

An ionic compound is considered as an ionic liquid herein when it is inthe liquid state at least in a temperature range from −10° C. to +50° C.Preferred ionic liquids are in the liquid state at least from −30° C. to+70° C., and the most preferred ionic liquids are in the liquid state inan even broader temperature range such as from −70° C. to +150° C.

The properties of ionic liquids can be modified and adapted to theparticular needs by varying the chemical structure. Typically, ionicliquids are thermally stable, have wide liquid regions, a high heatcapacity and nearly no vapour pressure. Most of them are incombustible.They can be even used as flame retardants. Reference is made to US2011/0073331 A1 disclosing ionic liquid flame retardants, and quotingliterature disclosing preparation methods (paragraph 0127).

As indicated above, the ionic liquids used in the present inventionshould be in the liquid state at a low temperature, preferably down to−30° C. or even below. Such ionic liquids are salts consisting oforganic cations and organic or inorganic anions, and both cations andanions are bulky and preferably asymmetric. As a general rule, themelting temperature decreases with increasing bulkiness and decreasingsymmetry of cations and anions. Combinations of highly bulky andasymmetric cations and anions may not freeze down to temperatures as lowas −120° C. Many ionic liquids are available which are liquid at −70° C.and above.

Suitable cations are, for example, imidazolium, pyrrolidinium, ammonium,choline, pyridinium, pyrazolium, piperidinium, phosphonium, andsulfonium cations. The cations may or may not have substituents.Particularly, the cations may have one or more substituents, for examplealkyl side chains such as methyl or butyl side chains. The substitutionmay be symmetric or asymmetric.

Suitable anions include dimethylphosphate, methylsulfate,trifluoromethylsulfonate, bis(trisfluoromethylsulfonyl)imide, chloride,bromide, iodide, tetrafluoroborate, and hexafluorophosphate. In the caseof “small” anions such as chloride, bromide, and iodide, particularlybulky cations can be selected, in order to provide for the desired lowtemperature liquidity.

Some exemplary ionic liquids are

-   butyltrimethylammoniumbis(trifluoromethylsulfonyl)imide    ([Me3BuN]TFSI)-   1-butyl-3-methylimidazoliumtrifluoromethanesulfonate (BMImOTf),-   1-butyl-3-methylimidazoliumdimethylphosphate (BMImPO₄Me₂),-   1-butyl-3-methylimidazoliummethylsulfate (BMImSO₄Me),-   1,1-butylmethylpyrrolidiniumbis(trifluoromethylsulfonyl)imide    (BmpyrTFSI),-   1,3-dimethylimidazoliumdimethylphosphate (MMImPO₄Me₂),-   1,3-dimethylimidazoliummethylsulfate (MMImSO₄Me).

The ionic liquids usable herein are, however, not particularly limited.It is only required that they are liquid and stable (i.e. they do notdecompose) in the desired temperature range. Of course, the ionicliquids must not react with any constituents of the oxygen generatingcomposition. The ionic liquids may be used singly or in combinations oftwo or more. Thus, in exemplary embodiments, this invention uses ionicliquid formulations. Such formulations may contain further additiveswhich do not detrimentally interfere with the peroxide decompositionreaction.

As an oxygen source, peroxide compounds, in particular solid hydrogenperoxide adduct compounds are used. Solid hydrogen peroxide adductcompounds constitute suitable and stable substitutes for liquid hydrogenperoxide, are easily storable, long term stable and safe to work with.Exemplary oxygen sources are alkalipercarbonates, e.g. sodiumpercarbonate (Na2CO3×1.5H2O2), alkaliperborates, e.g. sodium perborate(NaBO3×4H2O, NaBO3×H2O), and urea hydrogen peroxide (UHP). In UHP ureaand hydrogen peroxide are present in a molar ratio of about 1:1.

The peroxide compounds are not particularly limited, as long as they arestable under usual storage conditions, preferably also at elevatedtemperatures for example in the vicinity of a fire. The peroxidecompounds can be soluble or partially soluble or insoluble in the ionicliquids. The peroxide compounds can be used singly or in combinations oftwo or more; i.e. as oxygen source formulations. Such formulations maycontain further additives which do not detrimentally interfere with theperoxide decomposition reaction.

The decomposition reaction of the peroxide compound is catalyzed bymetal oxide compounds. Suitable metal oxide compounds are, for example,those which are known to catalyze the decomposition of peroxides inaqueous solutions.

Generally speaking, metal oxide compounds catalyzing peroxidedecomposition in compositions comprising ionic liquids, are oxides ofone single metal or of two or more different metals. The metal or themetals are selected from the group which consists of the elements ofgroups 2 to 14 of the periodic table of the elements. The periodic tablehas 18 groups (see: Pure and Applied chemistry, vol. 60, 3, pages431-436).

In exemplary embodiments the metal oxide compound is an oxide of one ormore metals belonging to the fourth period of the periodic table of theelements. In an alternative embodiment, the metal oxide compound is anoxide comprising, in addition to one or more metals belonging to thefourth period, one or more metal(s) belonging to the second and/or thirdand/or fifth and/or sixth period(s).

In further exemplary embodiments, the metal oxide compound is an oxideof one or more metals belonging to the fifth and/or sixth period of theperiodic table.

In all embodiments, each metal may be present in one single oxidationstate or in different oxidation states.

The metal oxide compounds may be used singly or in combinations of twoor more different metal oxide compounds, i.e. metal oxide formulationsmay be used.

Many metal oxide compounds are transition metal oxides.

Such transition metal oxides may contain one transition metal, and mayas well contain two or more different transition metals. Each transitionmetal may be present in one single or in different oxidation states. Inaddition, the transition metal oxides may contain one or morenon-transition metals. The transition metal oxides may be used singly orin combinations of two or more different transition metal oxides.

Exemplary transition metal oxide catalysts include oxides of manganese,cobalt, chromium, silver and copper, and mixed oxides of iron andanother transition metal such as cobalt, copper, nickel, or manganese,mixed oxides of manganese and another transition metal such as cobalt,nickel, or copper, and mixed oxides containing nickel and cobalt.

As regards structural types, spinel type oxides, ilmenite type oxides,and perovskite type oxides may be specifically mentioned.

As exemplary compounds catalyzing the peroxide decomposition reactionmay be mentioned: manganese (IV) oxide (MnO2), cobalt (II, III) oxide(Co3O4), chromium (VI) oxide (CrO3), silver (I) oxide (Ag2O), and copper(II) oxide (CuO), as well as spinel type mixed metal oxides like cobaltiron oxide (CoxFe3-×O4, with 0≤×≤3), such as CoFe2O4, Co1.5Fe1.5O4, andCo2FeO4, copper iron oxide (CuxFe3-×O4, with 0≤×≤3), such as CuFe2O4,nickel iron oxides (NixFe3-×O4, with 0≤×≤3), manganese iron oxides(MnxFe3-×O4, with 0≤×≤3), copper manganese oxides such as Cu1.5Mn1.5O4,cobalt manganese oxides such as Co2MnO4, nickel cobalt oxides such asNiCo2O4, as well as ilmenite type oxides like nickel manganese oxidessuch as NiMn03 or oxides containing more than two transition metals, forexample LaFexNil-×O3, with 0≤×≤1, or LaxSrl-×MnO3 with 0≤×≤1.

Transition metals as understood herein are those elements which have anincomplete d-shell, or which may form ions having an incomplete d-shell,including lanthanides and actinides. It goes without saying that onlyoxides may be used which undergo a redox reaction with hydrogenperoxide.Zincoxide, for example, may not be used, although zinc constitutes atransition metal. It is, however, stressed that the metal oxidecompounds are not limited to transition metal oxides. Rather, the metaloxide compounds may be oxides of main group metals, such as PbO2, oroxides of main group metals and transition metals in combination, suchas La0.5Sr0.5MnO3.

The compositions for generating oxygen may comprise from about 10 to 80weight % of one or more oxygen sources, from about 20 to 80 weight % ofone or more ionic liquids, and from more than 0 up to about 20 weight %of one or more metal oxide catalysts. In exemplary embodiments, theoxygen source or mixture of oxygen sources constitutes from 50 to 70weight %, the ionic liquid or mixture of ionic liquids constitutes from30 to 60 weight %, and the metal oxide catalyst or mixture of metaloxide catalysts constitutes from more than 0 up to about 10 weight % ofthe composition. In some embodiments, the oxygen source may constituteup to 98 weight % of the composition, with the amounts of ionic liquidand catalyst being present in amounts as low as about 1% by weight,each. Optionally, further constituents may be present, for examplesilicon dioxide (as a heat sink), resorcinol (as a radical scavenger),2-methylhydrochinone, eugenol, phenol, and 4-propylphenol, all of whichreduce the peroxide decomposition rate. In some embodiments, the amountsof such additional constituents do not exceed about 20 weight % of thecomposition. All constituents together add up to 100 weight %.

In the context herein, the term “composition” includes conditionswherein all constituents of the composition are mixed, i.e. are incontact with each other, as well as conditions wherein the constituentsare not in contact with each other, or wherein at least not allconstituents are in contact with each other. It must be considered thata mixture comprising an ionic liquid, a peroxide compound dissolved ordispersed therein, and a metal oxide catalyst, is not stable. Rather,the decomposition of the peroxide compound starts as soon as the metaloxide catalyst comes into contact with the peroxide compound, in theionic liquid, or at least shortly thereafter. Therefore, theconstituents of the composition for generating oxygen must be stored ina condition wherein the catalyst cannot trigger the release of oxygenfrom the peroxide compound. This can be achieved by providing thecomposition for generating oxygen in the form of a “kit of parts”, i.e.as a combination of at least two components, the two componentscomprising the at least one oxygen source, the at least one ionicliquid, and the at least one metal oxide compound. In the at least twocomponents, at least one of the three constituents (the oxygensource(s), the ionic liquid(s), and the metal oxide compound(s)) is notin contact with the other constituents of the composition for generatingoxygen.

According to a first embodiment, the composition comprises a firstcomponent and a second component, the first component comprising theoxygen source and the ionic liquid, and the second component comprisingthe metal oxide.

According to a second embodiment, the composition comprises a firstcomponent and a second component, the first component comprising themetal oxide and the ionic liquid, and the second component comprisingthe oxygen source.

According to a third embodiment, the composition comprises a firstcomponent and a second component, the first component comprising theoxygen source and the metal oxide, and the second component comprisingthe ionic liquid.

According to a fourth embodiment, the composition comprises threecomponents, the first component comprising the oxygen source, the secondcomponent comprising the ionic liquid, and the third componentcomprising the transition metal oxide.

Accordingly, an exemplary method for generating oxygen comprisesproviding at least one oxygen source, providing at least one ionicliquid, providing at least one metal oxide compound, wherein the oxygensource is a peroxide compound, the ionic liquid is in the liquid stateat least in the temperature range from −10° C. to +50° C., the metaloxide compound is an oxide of one single metal or of two or moredifferent metals, said metal(s) being selected from the metals of groups2 to 14 of the periodic table of the elements, and contacting the atleast one oxygen source, the at least one ionic liquid, and the at leastone metal oxide compound.

According to a first embodiment, the oxygen source and the ionic liquidare provided as a first component, the metal oxide compound is providedas a second component, and the step of contacting comprises mixing thefirst component and the second component.

According to a second embodiment, the metal oxide compound and the ionicliquid are provided as a first component, the oxygen source is providedas a second component, and the step of contacting comprises mixing thefirst component and the second component.

According to a third embodiment, the oxygen source and the metal oxidecompound are provided as a first component, and the ionic liquid isprovided as a second component, and the step of contacting comprisesmixing the first component and the second component.

According to a fourth embodiment, the oxygen source is provided as afirst component, the ionic liquid is provided as a second component, themetal oxide compound is provided as a third component, and the step ofcontacting comprises mixing the first component, the second componentand the third component.

When the oxygen source and the metal oxide compound are provided as onesingle component, i.e. in an admixed state, both the oxygen source andthe metal oxide compound should be thoroughly dried before mixing.Otherwise, the oxygen source will be decomposed inadvertently. In theabsence of any mediator, for example water or an ionic liquid, the solidoxygen source and the solid metal oxide compound constitute long termstable mixtures.

An exemplary device for generating oxygen by the above method isspecifically adapted for housing the components of the composition forgenerating oxygen in a physically separated state, and bringing theminto physical contact once generation of oxygen is desired.

An exemplary device comprises at least one reaction chamber. Thereaction chamber may have one single compartment or two compartmentsseparated from one another by a membrane or another means which can beeasily destroyed, for example a thin glass plate or a thin metal orplastic foil. Alternatively, the reaction chamber may contain at leastone receptacle for receiving one or two of the essential constituents ofthe composition for generating oxygen, i.e. one or two of the at leastone oxygen source, the at least one ionic liquid, and the at least onemetal oxide compound. By placing at least one of the constituents in asealable receptacle, while the other constituents are outside thereceptacle, or alternatively, by placing at least one of theconstituents of the composition for generating oxygen in a firstcompartment of the reaction chamber, while the other constituents areplaced in a second compartment of the reaction chamber, the constituentsare maintained physically separated, and a decomposition reaction of theperoxide compound is prevented.

In order to allow the generation of oxygen, physical contact of theconstituents of the composition for generating oxygen must beestablished. This can be achieved, for example, by destroying themembrane or foil or other means separating the first compartment and thesecond compartment of the reaction chamber, or by destroying thereceptacle containing at least one of the constituents of thecomposition for generating oxygen. The membrane or other separatingmeans may be, for example, destroyed by a cutting edge of a cuttingdevice arranged in one of the compartments of the reaction chamber, andthe receptacle arranged within a reaction chamber containing only onecompartment may be, for example, destroyed by a solid plate, a grid, ora firing pin. Both the cutting device having the cutting edge and thesolid plate or grid are moved upon activation by an actuator, forexample a spring mechanism. The actuator may be actuated, for example,by a person requiring oxygen or may be actuated automatically, once alow oxygen condition is sensed by an oxygen sensor.

Once contact of the constituents has been established, oxygen generationbegins promptly or somewhat delayed, depending on the state of theconstituents as will be described below. The oxygen leaves the reactionchamber via means allowing the passage of oxygen, while otherwisesealing the reaction chamber, for example a gas permeable membrane, orany other structure which is gas permeable, but liquid tight, e.g. afrit or a molecular sieve. When the reaction chamber is arranged withina container, the oxygen may be released into a head space of thecontainer, and leave the container through an oxygen outlet.

In an exemplary embodiment, the device for generating oxygen comprisesmore than one reaction chamber, and the at least two reaction chambersare arranged within a common container. Each reaction chamber may beprovided, individually, with means for establishing physical contact ofthe constituents of the composition for generating oxygen, oralternatively, a common such means may be provided for a plurality ofthe reaction chambers or for all reaction chambers. The oxygen generatedin each reaction chamber is released into a common head space of thecontainer, and leaves the container through an oxygen outlet.

The embodiment comprising a plurality of reaction chambers allows thatoxygen can be provided over a particularly long time period by chargingthe reaction chambers with compositions for generating oxygen havingdifferent oxygen release profiles. Alternatively, such compositionshaving different oxygen release profiles may be also charged into onesingle reaction chamber, thus providing oxygen over a long time period.It is readily apparent that such device for generating oxygen havingonly one reaction chamber is of a very simple construction. Simpleconstructions are typically the most reliable ones.

It has been found by the present inventors, that the course of thedecomposition reaction of the peroxide compound can be influenced byvarious factors.

The nature of the peroxide compound has no or almost no influence, i.e.all tested peroxide compounds have been found to behave equivalently.The nature of the ionic liquid has been found to have some influence onthe time point of onset of the reaction and on the reaction rate. Thisinfluence is due to solubility differences of the oxygen source in theionic liquid. The decomposition reaction proceeds faster in case of anoxygen source which is highly soluble in the ionic liquid than in thecase of an oxygen source having poor or no solubility in the ionicliquid.

The amount of metal oxide catalyst has more influence on the peroxidedecomposition reaction. The reaction profile of the decompositionreaction depends on the concentration of the metal oxide catalyst, i.e.the reaction rate, the time point of onset of the reaction, and thereaction temperature is different for different metal oxide catalystconcentrations. The decomposition reaction rate increases withincreasing amount of catalyst.

What has the greatest influence on the decomposition reaction profile,is the surface area of the peroxide compound exposed to the metal oxidecatalyst. The reaction rate can be considerably varied by reducing orenlarging the surface area of peroxide compound. The reaction isparticularly fast, when the peroxo compounds are present in the form offine particles. Small particles can be easily and quickly dissolved inthe ionic liquid, and even in the case of low solubility in the ionicliquid, small particles have a relatively larger surface area than anequal weight of coarser particles.

If it is desired to extend the time span of oxygen generation, or if itis desired to delay the onset of the decomposition reaction, theperoxide compound may be compressed into powder compacts. Powdercompacts may differ in shape (having, for example, cylindrical orrectangular block shapes), in dimensions, in degree of compaction (whichincreases with increasing compaction pressure), and in weight. It hasbeen found that the weight directly influences the amount of oxygengenerated, i.e. the reaction is scalable. The reaction rate, however, isindependent of the weight and the shape of the powder compacts and alsoquite independent of the dimensions of the powder compacts.

A strong influence has been found for the degree of compaction. Highcompaction pressures clearly delayed the onset of the reaction and/orextended the time period of oxygen generation. The reason is that highcompaction pressure results in high density of the powder compacts,resulting in low porosity of the powder compacts. Powder compacts havingmany open pores at the surfaces thereof can be easily and quicklypenetrated by the ionic liquid, while powder compacts having only fewopen pores at the surfaces thereof do not allow fast penetration of theionic liquid into the bulk of the powder compact. Therefore, contactwith the metal oxide catalyst is delayed in the case of powder compactshaving a high degree of compaction, and the delay increases withincreasing degree of compaction.

In exemplary embodiments, the ionic liquids described above are used asdispersants or solvents and as heat sinks in the compositions forgenerating oxygen described above.

The disclosed uses, methods and devices may take advantage of any of thematerials described above in relation to compositions and vice versa.

All references herein to “comprising” should be understood to encompass“including” and “containing” as well as “consisting of” and “consistingessentially of”.

The term “a” means “at least one”.

BRIEF DESCRIPTION OF THE DRAWINGS

The invention will be further illustrated by the following non limitingexamples with reference to the accompanying drawings, wherein:

FIG. 1 is a graph illustrating reproducibility of oxygen release from acomposition of the present invention,

FIG. 2 is a graph illustrating oxygen release from different amounts ofUHP through metal oxides in MMImPO4Me2,

FIG. 3 is a graph illustrating reaction temperatures for thedecomposition reactions illustrated in FIG. 2,

FIGS. 4a, 4b are graphs illustrating oxygen release from 1 g UHP indifferent ionic liquids by catalytic amounts of manganese (IV) dioxide,

FIG. 5 is a graph illustrating oxygen release from 1 g UHP in MMImPO4Me2by different metal oxides,

FIG. 6 is a graph illustrating oxygen evolution from 10 g UHP usingdifferent catalyst concentrations,

FIG. 7 is a graph illustrating oxygen release from mixtures of SPC andUHP in ionic liquids,

FIG. 8 is a graph illustrating oxygen release from 1 g UHP in MMImPO4Me2by different metal oxides,

FIG. 9 is a graph illustrating oxygen release from 2 g UHP usingdifferent catalysts,

FIG. 10 is a graph illustrating oxygen release from different amounts ofUHP through a mixed metal oxide in MMImPO4Me2,

FIG. 11 is a graph illustrating reaction temperatures of thedecomposition reactions illustrated in FIG. 10,

FIG. 12 illustrates oxygen release from 1 g UHP in different ionicliquids by catalytic amounts of mangenese (IV) dioxide,

FIGS. 13 and 14 are graphs illustrating oxygen release from 2 g UHPusing different catalysts and different concentrations,

FIG. 15 illustrates oxygen release from UHP, SPC and mixtures thereofthrough Co2FeO4 in MMimPO4Me2,

FIG. 16 illustrates oxygen release from 1 g UHP powder and 1 g UHPpowder compact,

FIG. 17 illustrates oxygen release from 2 g UHP powder and two different2 g UHP powder compacts, and

FIGS. 18 to 22 schematically illustrate several embodiments of devicesfor generating oxygen from compositions according to the invention.

DETAILED DESCRIPTION

In all graphs illustrating oxygen evolution or reaction temperature,oxygen evolution (or reaction temperature, respectively) is plottedagainst runtime, wherein runtime is the time which starts running at thetime point of contacting the oxygen source (formulation) and the ionicliquid (formulation) comprising an active ionic liquid.

EXAMPLE 1

10.0 g urea hydrogen peroxide adduct (UHP) were added to a dispersion of2 mol % (relative to UHP) MnO2 (0.184 g) in 5.0 g1,3-dimethylimidazoliumdimethylphosphate (MMImPO4Me2), contained in aglass flask. The flask was closed, and the oxygen volume released by thedecomposition reaction was measured with a drum gas meter. Theexperiment was repeated three times. As FIG. 1 shows, the reactionprofile was substantially identical in all experiments, proving that thedecomposition reaction was reliably reproducible.

EXAMPLE 2

Urea hydrogen peroxide (UHP) adduct in the amounts listed in table 1 wasadded to dispersions of 2 mol % (relative to UHP) MnO2 in MMImPO4Me2(amounts listed in table 1) contained in a glass flask. The flask wasclosed, and the oxygen volume released by the decomposition reaction wasmeasured with a drum gas meter. In addition, the reaction temperaturewas measured. The results are illustrated in FIGS. 2 and 3.

FIG. 2 shows that when varying amounts of peroxide compound are added toequivalently varying amounts of ionic liquid and catalyst, the amount ofoxygen released by the decomposition reaction increases proportionally,thus proving that the decomposition reaction is scalable for differentsizes of devices for generating oxygen.

FIG. 3 shows that the reaction temperatures increase with increasingamounts of reaction mixture, but remain well below 150° C. even for thesample containing 20 g UHP.

TABLE 1 mass peroxide peroxide mass MnO2 reaction adduct adduct mass ILcatalyst volume time UHP 2.5 g 1.25 g 0.046 g 300 cm³ 6.1 min UHP 5 g2.5 g 0.092 g 700 cm³ 5.9 min UHP 10 g 5 g 0.184 g 1455 cm³ 5.9 min UHP20 g 10 g 0.368 g 2970 cm³ 6.1 min

EXAMPLE 3

1.0 g urea hydrogen peroxide adduct compound (UHP) was added to adispersion of 5 mol % (relative to UHP) MnO2 catalyst in 0.5 g ofdifferent ionic liquids (IL) contained in a glass flask each. The ionicliquids used are listed below. The flask was closed, and the oxygenvolume released by the decomposition reaction was measured with a drumgas meter. The results are shown in FIGS. 4a and 4b . FIGS. 4a and 4breveal that all ionic liquids worked well. The reaction speed isinfluenced to some extent by the particular ionic liquid used.

Ionic liquids:

-   butyltrimethylammoniumbis(trifluoromethylsulfonyl)imide    ([Me3BuN]TFSI)-   1-butyl-3-methylimidazoliumtrifluoromethanesulfonate (BMImOTf),-   1-butyl-3-methylimidazoliumdimethylphosphate (BMImPO₄Me₂),-   1-butyl-3-methylimidazoliummethylsulfate (BMImSO₄Me),-   1,1-butylmethylpyrrolidiniumbis(trifluoromethylsulfonyl)imide    (BmpyrTFSI),-   1,3-dimethylimidazoliumdimethylphosphate (MMImPO₄Me₂),-   1,3-dimethylimidazoliummethylsulfate (MMImSO₄Me).

EXAMPLE 4

1.0 g urea hydrogen peroxide adduct compound were added to dispersionsof different metal oxide catalysts in 0.5 g MMImPO4Me2 contained in aglass flask. The flask was closed, and the oxygen volume released by thedecomposition reaction was measured with a drum gas meter. The catalystsused are listed in table 2, and the reaction profiles are shown in FIG.5.

FIG. 5 reveals that both the onset of the reaction and the reactionvelocity depend on the particular catalyst used. While in the case ofCrO3 the reaction starts immediately after contacting peroxide compoundand catalyst, and is finished within a few seconds, in the case of theother catalysts, the onset of the reaction is somewhat delayed, and thereaction velocity is slower.

TABLE 2 peroxide metal oxide adduct catalyst mass catalyst volume UHPCo₃O₄ 0.128 g 145 cm³ UHP CrO₃ 0.053 g 200 cm³ UHP MnO₂ 0.092 g 140 cm³UHP PbO₂ 0.051 g 142 cm³ UHP Fe₃O₄ 0.123 g  18 cm³

EXAMPLE 5

10.0 g UHP were added to dispersions of different amounts of MnO2catalyst in 7.5 g MMImPO4Me2 contained in a glass flask. The amounts andconcentrations (relative to UHP) of MnO2 are indicated in table 3. Theflask was closed, and the oxygen volume released by the decompositionreaction was measured with a drum gas meter. The reaction profiles areshown in FIG. 6.

It is evident from FIG. 6 that the catalyst concentration can be variedover a broad range, and that it exerts a strong influence both on thereaction velocity and on the amount of oxygen released. The reactionvelocity dramatically increases with increasing catalyst concentration.

TABLE 3 peroxide catalyst adduct concentration mass catalyst volumeTime 1) UHP 1 mole % 0.092 g  863 cm³ 55.0 min UHP 2 mole % 0.184 g 1253cm³ 24.6 min UHP 4 mole % 0.368 g 1488 cm³ 5.7 min UHP 8 mole % 0.736 g1365 cm³ 2.0 min 1) “time” means time until complete release of allavailable oxygen

EXAMPLE 6

Urea hydrogen peroxide (UHP), sodiumpercabonate (SPC), and mixturesthereof in the amounts listed in table 4 were added to dispersions of 2mol % (relative to the peroxide compound) MnO2 in 5.0 g MMImPO4Me2. Thereaction vessel was closed, and the oxygen volume released by thedecomposition reaction was measured with a drum gas meter. The resultsare illustrated in FIG. 7.

FIG. 7 illustrates that the nature of the peroxide compound has onlylittle influence on the course of the decomposition reaction. Thesomewhat longer reaction time and reduced oxygen generation can beattributed to the somewhat lower solubility of SPC, as compared to UHP,in the particular ionic liquid used in this experiment.

TABLE 4 mass UHP mass SPC mass MnO₂ volume time  10 g 0 0.184 g 1458 cm³5.97 min 7.5 g 4.2 g 0.184 g 1343 cm³ 5.53 min 6.7 g 5.4 g 0.184 g 1290cm³ 4.07 min 0  10 g  0.11 g 1005 cm³ 6.60 min

EXAMPLE 7

2 g urea hydrogen peroxide adduct (UHP) were added to dispersions of 5mol % (relative to UHP) of different mixed metal oxide catalysts in 1.0g MMImPO4Me2 contained in a glass flask. The flask was closed, and theoxygen volume released by the decomposition reaction was measured with adrum gas meter. All catalysts were mixed cobalt iron oxides, as listedin table 5. The reaction profiles are shown in FIG. 8

FIG. 8 reveals that all tested cobalt iron oxide catalysts behaved verysimilar. There was almost no difference in reaction velocity, time pointof onset of the reaction, and oxygen volume generated.

TABLE 5 peroxide adduct metal oxide mass catalyst volume UHP CoFe₂O₄0.249 g 295 cm³ UHP Co_(1.5)Fe_(1.5)O₄ 0.251 g 290 cm³ UHP Co₂FeO₄ 0.253g 290 cm³

EXAMPLE 8

2 g urea hydrogen peroxide adduct (UHP) were added to dispersions of 5mol % (relative to UHP) of different mixed metal oxide catalysts in 1 gMMImPO4Me2 contained in glass flasks. The flasks were closed, and theoxygen volume released by the decomposition reactions was measured witha drum gas meter. The particular catalyst used are listed in table 6,and the reaction profiles are shown in FIG. 9.

In this example, in contrast to the results obtained in example 7,differences were found between the individual mixed metal oxidecatalysts. While not wishing to be bound by this theory, it is believedthat the different findings in example 7 and example 8 can be attributedto the fact that the mixed metal oxide catalysts used in example 7contained the same transition metals, and only the relative amounts werevaried, while the mixed metal oxide catalysts used in example 8contained different transition metals, i.e. each mixed metal oxidecontained a different combination of transition metals.

TABLE 6 catalyst catalyst mass volume CuFe₂O₄ 0.254 g 243 cm³Cu_(1.5)Mn_(1.5)MnO₄ 0.315 g 385 cm³ NiMnO₃ 0.172 g 285 cm³ NiCo₂O₄0.256 g 295 cm³ Co₂MnO₄ 0.252 g 265 cm³ La_(0.5)Sr_(0.5)MnO₃ 0.125 g 223cm³ LaFe_(0.25)Ni_(0.75)O₃ 0.245 g  45 cm³

EXAMPLE 9

Urea hydrogen peroxide adduct compound in the amounts listed in table 7were added to dispersions of 2 mol % (relative to UHP) Co1.5Fe1.5O4 incorresponding amounts (see table 7) of MMImPO4Me2 contained in glassflasks. The flasks were sealed, and the oxygen volume released by thedecomposition reaction was measured with a drum gas meter. In addition,the reaction temperatures were measured. The results are illustrated inFIGS. 10 and 11.

FIG. 10 shows that when varying amounts of peroxide compound are addedto equivalently varying amounts of ionic liquid and mixed metal oxidecatalyst, the amount of oxygen released increases proportionally, thusproving that the decomposition reaction is scalable for different sizesof devices for generating oxygen.

FIG. 11 shows that the reaction temperatures increase with increasingamounts of the reaction mixtures. However, the reaction temperaturesalways remained below 110° C. In the case of example 2 wherein manganese(IV) oxide was used as a catalyst, i.e. an oxide containing only onesingle transition metal rather than mixed metals, was used as acatalyst, the maximum reaction temperatures appeared to be somewhathigher, thus suggesting a tendency towards lower reaction temperatureswith mixed metal oxide catalysts than with single metal oxide catalysts.

TABLE 7 peroxide mass mass adduct peroxide mass IL catalyst volume timeUHP 2.5 g 1.25 g 0.046 g 300 cm³ 6.1 min UHP 5 g 2.5 g 0.092 g 700 cm³5.9 min UHP 10 g 5 g 0.184 g 1455 cm³ 5.9 min UHP 20 g 10 g 0.368 g 2970cm³ 6.1 min

EXAMPLE 10

1.0 g urea hydrogen peroxide adduct was added to dispersions of 10 mol %(relative to UHP) Fe1.5Co1.5O4 in 0.5 g of different ionic liquidscontained in glass flasks. The ionic liquids used are listed below. Theflasks were closed, and the oxygen volume released by the decompositionreactions were measured with a drum gas meter. The results are shown inFIG. 12.

FIG. 12 reveals that all ionic liquids worked well. The reactionvelocity was influenced to some extent by the particular ionic liquidused.

Used ionic liquids:

-   1-butyl-3-methylimidazoliumtrifluoromethanesulfonate (BMImOTf)-   1,1-butylmethylpyrrolidiniumbis(trifluoromethylsulfonyl)imide    (BMpyrTFSI)-   1,3-dimethylimidazoliumdimethylphosphate (MMImPO₄Me₂)-   1,3-dimethylimidazoliummethylsulfate (MMImSO₄Me)

EXAMPLE 11

2 g urea hydrogen peroxide adduct (UHP) were added to dispersions ofdifferent amounts of NiCo2O4 catalyst and CoFe2O2 catalyst,respectively, in 1 g MMImPO4Me2 in a glass flask. Amounts andconcentrations (relative to UHP) of the catalysts are indicated in table8. The flasks were closed, and the oxygen volume released by thedecomposition reaction was measured with a drum gas meter. The reactionprofiles for NiCo2O4 are shown in FIG. 13, and the reaction profiles forCoFe2O4 are shown in FIG. 14.

It is evident from FIGS. 13 and 14 that the catalyst concentration canbe varied over a broad range and exerts a strong influence both on thereaction velocity and on the amount of oxygen released. The reactionvelocity dramatically increases with increasing catalyst concentration.

TABLE 8 per- concen- oxide tration mass adduct catalyst catalystcatalyst volume time UHP NiCo₂O₄ 2 mol % 0.152 g 92 cm³ 41.1 min UHPNiCo₂O₄ 5 mol % 0.382 g 290 cm³ 12.5 min UHP NiCo₂O₄ 8 mol % 0.612 g 305cm³ 9.1 min UHP CoFe₂O₄ 1 mol % 0.050 g 67 cm³ 47.6 min UHP CoFe₂O₄ 2mol % 0.100 g 203 cm³ 41.5 min UHP CoFe₂O₄ 5 mol % 0.250 g 303 cm³ 3.9min UHP CoFe₂O₄ 8 mol % 0.399 g 293 cm³ 2.3 min

EXAMPLE 12

Urea hydrogen peroxide adduct (UHP), sodium percarbonate (SPC), andmixtures thereof in the amounts listed in table 9 were added todispersions of 0.505 g Co₂FeO₄ in 5 g MMImPO₄Me_(2.) The reactionvessels were closed, and the oxygen volume released by the decompositionreactions were measured with a drum gas meter. Amounts of oxygengenerated as well as the reaction times are shown in FIG. 15.

TABLE 9 mass UHP mass SPC volume time   2 g 0 260 cm³ 5.9 min 1.3 g 1.0g 275 cm³ 6.2 min 0   2 g 265 cm³ 7.6 min

FIG. 15 illustrates the nature of the peroxide compound has only littleinfluence on the course of the decomposition reaction.

EXAMPLE 13

In a first experiment, 10 g urea hydrogen peroxide adduct (UHP) inpowder form were added to a dispersion of 0.184 g MnO2 in 5.0 gMMImPO4Me2 contained in a glass flask.

In a second experiment, 10 g of the same UHP powder which was used inexample 1, were pressed into a powder compact by applying a compactionpressure of 38 MPa. The pellet was added to a dispersion of MnO2 inMMIm-PO4Me2, as used in experiment 1.

The flasks were closed, and the oxygen volumes released by thedecomposition reactions were measured with a drum gas meter. The resultsare shown in table 10 and FIG. 16.

It is obvious that the reaction velocity was considerably reduced andthe time of oxygen production considerably extended, respectively, bycompacting the hydrogen peroxide adduct compound.

TABLE 10 peroxide compaction adduct (form) mass pressure volume time UHP(powder) 10 g — 1460 cm³  7 min UHP (powder 10 g 38 MPa 1120 cm³ 58 mincompact)

EXAMPLE 14

In a first experiment 2 g urea hydrogen peroxide adduct (UHP) in powderform were added to a dispersion of 0.074 g Co1.5Fe1.5O4 in 1.0 gMMIm-PO4Me2 contained in a glass flask.

In a second experiment, 2 g of the same UHP powder which was used in thefirst experiment, were pressed into a powder compact by applying acompaction pressure of 38 MPa. The pellet was added to a dispersion ofCo1.5Fe1.5O4 in MMImPO4Me2 as used in experiment 1.

In a third experiment, 2 g of the same UHP powder which was used in thefirst and the second experiment, were pressed into a powder compact byapplying a compaction pressure of 220 MPa. The pellet was added to adispersion of Co1.5Fe1.5O4 in MMimPO4Me2 as used in experiments 1 and 2.

The flask was closed, and the oxygen volume released by thedecomposition reactions was measured with a drum gas meter. The resultsare shown in table 11 and FIG. 17. It is obvious that the reactionvelocity was considerably reduced and the time of oxygen generation wasconsiderably extended, respectively, by compacting the hydrogen peroxideadduct compound into pellet form. The effect increases with increasingcompaction pressure.

TABLE 11 peroxide compaction mass adduct (form) mass pressureCo_(1.5)Fe_(1.5)O₄ volume time UHP (powder) 2 g — 0.074 g 280 cm³  7 minUHP (powder 2 g  38 MPa 0.074 g 263 cm³ 29 min compact) UHP (powder 2 g220 MPa 0.074 g 142 cm³ 90 min compact)

Thus, examples 13 and 14 prove that reducing the accessible surface areaof the peroxide compound, for example by pressing, constitutes a simplemeasure for extending the time of oxygen release, i.e. for extending thetime span wherein breathable oxygen is available.

An exemplary device for generating oxygen from compositions as describedabove which use ionic liquids for dissolving or dispersing a hydrogenperoxide adduct compound as an oxygen source, and for dispersing acatalyst and bringing the catalyst into contact with the oxygen source,is specifically designed. An exemplary device for generating oxygen hasat least one reaction chamber for storing the composition in a conditionwhere not all constituents of the composition are in physical contact.Such physical contact of all constituents of the composition isestablished at the very moment when oxygen is required. The device isequipped with suitable means for allowing the constituents to contacteach other at that very moment. Furthermore, the device allows that thegenerated oxygen exits the reaction chamber. Some exemplary devices areillustrated in FIGS. 18 to 22, wherein like reference numerals designatelike components. The description of such exemplary embodiments shall notbe construed as limiting the invention in any manner.

FIG. 18 illustrates a device for generating oxygen 1 having one singlereaction chamber 2 for storing the composition for generating oxygen. Insuch a single reaction chamber 2 at least one of the constituents of thecomposition for generating oxygen must be enclosed in a receptacle inorder to avoid contact with the remaining constituents of thecomposition contained in the reaction chamber 2. In the embodiment shownin FIG. 18, two receptacles 5, 6 are arranged in the reaction chamber.Receptacle 5 contains an intimate mixture of the oxygen source 7 and thedecomposition catalyst 9, for example in powder form or compressed intopellets, in a thoroughly dried condition. Receptacle 6 contains theionic liquid 8. Alternatively, there may be only one receptacle forenclosing the peroxide/catalyst mixture, while the ionic liquid is“free” within reaction chamber 2, or ionic liquid 8 may be enclosedwithin a receptacle, while the peroxide/catalyst mixture is not enclosedin a separate receptacle. It is, in principle, also possible to encloseonly the catalyst within a separate receptacle, while the ionic liquidand the peroxide are not enclosed. It is only necessary to avoid contactbetween all three constituents during storage of the device forgenerating oxygen.

It is desirable to store the peroxide 7, the ionic liquid 8 and thecatalyst 9 within the reaction chamber 2 in such an arrangement that allconstituents will be able to get intimately mixed once oxygen generationis required. When, for example, the catalyst and the ionic liquid areprovided in one receptacle, and the peroxide in another receptacle, thecatalyst may settle within the ionic liquid during storage, and propermixing with the peroxide may be inhibited. Quick and perfect mixing ofall constituents can be achieved when the peroxide and the catalyst areintimately mixed in advance in a dry condition, optionally compactedinto moulds, and filled either into the reaction chamber 2 or into aseparate receptacle 5 to be placed within the reaction chamber 2, andthe ionic liquid is provided in a separate receptacle 6. Placing theionic liquid in a separate receptacle, although this is not absolutelynecessary in a case where peroxide and catalyst are placed in areceptacle 5, constitutes an advantageous precautionary measure againstaccidental mixing of the constituents in case of receptacle 5 leakage orbreakage. Care must be taken, when UHP and catalyst are mixed, becauseUHP is highly hygroscopic.

In a situation where oxygen shall be generated, receptacle 5, orreceptacles 5 and 6, respectively, are destroyed by a breaking device18. In FIG. 18, breaking device 18 has the form of a plate, however,means for destroying the receptacle(s) are not limited to plates, andother means are known to persons skilled in the art, for example firingpins or grids. Movement of plate 18 can be achieved by a spring 19 oranother activation mechanism. During storage of the device forgenerating oxygen, spring 19 is under tension and holds plate 18 at aposition distant from receptacles 5, 6. Once the tension is released bya suitable trigger mechanism (not shown), spring 19 moves plate 18towards receptacles 5, 6, and plate 18 destroys receptacles 5, 6. Such atrigger may be, for example, pulling an oxygen mask towards a passengerin an airplane. Another exemplary trigger mechanism is an oxygen sensorsensing a low oxygen condition.

Receptacles 5, 6, and plate 18 are made from materials which guaranteethat receptacles 5, 6 will be broken or ruptured when hit by plate 18.Exemplary materials are plastic foils or glass for receptacles 5, 6, andthicker plastic material or metal for plate 18.

Destruction of receptacles 5, 6 causes mixing of peroxide, ionic liquid,and catalyst, and initiates oxygen generation. In order to allow thatthe oxygen exits reaction chamber 2, reaction chamber 2 has an opening.In the illustrated embodiment, the opening is sealed with a gaspermeable membrane 16. The opening may be at a different position thanshown in FIG. 18, or there may be more than one opening. This appliesanalogously to all devices for generating oxygen of the invention.

The oxygen generated in the devices of this invention may be passedthrough a filter or other purification means as known in the art. Thedevices may be equipped with such means.

The oxygen generating reaction is an only slightly exothermic process,and proceeds at low temperature, i.e. well below 150° C. Therefore,reaction chamber 2 does not need to resist high temperatures, and may bemade from lightweight, low melting materials such as plastic. Inaddition, any bulky insulation is not required. This is particularlyadvantageous in all cases where weight must be saved and/or space islimited, for example in the case of oxygen masks which shall beinstalled in an aircraft.

FIG. 19 illustrates an alternative embodiment of an exemplary device 1for generating oxygen. In the embodiment of FIG. 19, the reactionchamber 2 has two compartments, a first compartment 3, and a secondcompartment 4, which are separated by a gastight membrane 17. The firstcompartment 3 contains one or more constituents of the composition forgenerating oxygen. Compartment 3 is equipped with a cutting device 20having cutting edge 20′, and the cutting device is arranged in aposition that allows cutting edge 20′ to cut through membrane 17separating the first compartment 3 and the second compartment 4.

Compartments 3, 4 have openings sealed by membranes 15 and 16,respectively. Membranes 15, 16 are gas permeable, thus allowing theoxygen generated during the oxygen generating reaction to exit reactionchamber 2.

An activation mechanism 19, for example a spring, is provided for movingcutting device 20 towards membrane 17, and through membrane 17. Such amechanism is described in DE 10 2009 041 065 A1. As explained inconnection with FIG. 18, spring 19 is under tension during storage ofdevice 1, and once the tension is released by a trigger mechanism (notshown), spring 19 moves receptacle 5 towards membrane 17, cutting edge20′ destroys membrane 17, and first compartment 3 and second compartment4 are combined into one single reaction chamber 2.

In the embodiment illustrated in FIG. 19, a mixture of peroxide 7 andcatalyst 9 is contained in the first compartment 3, and ionic liquid 8is contained in second compartment 4. Upon destruction of membrane 17,the peroxide/catalyst formulation falls into the second compartment 4,and mixes with ionic liquid 8. The oxygen generated exits the reactionchamber 2 through membranes 15, 16.

Of course, it is also possible to place ionic liquid 8 into the firstcompartment 3 and the peroxide/catalyst formulation into the secondcompartment 4, or to use any other arrangement wherein at least one ofthe constituents is separated from the remaining constituents.

As a material for the cutting device 20, any material may be used whichmay cut membrane 17, for example a metal sheet. The first compartment 3and the second compartment 4 can be formed from the same materials asthe single reaction chamber 2 illustrated in FIG. 18.

Another embodiment of an inventive device 1 for generating oxygen isillustrated in FIG. 20. In the embodiment of FIG. 20, the reactionchamber 2 is equipped with an injection device 21, for example a syringeor another dosing device.

Reaction chamber 2 and injection device 21 are connected, or constituteseparate units which can be connected, to form one single unit. Anopening, or several openings, in the wall of reaction chamber 2 allowthat oxygen generated during the peroxide decomposition reaction exitsreaction chamber 2. The openings are sealed in the embodiment shown bygas permeable membranes 16. In the embodiment illustrated in FIG. 20,the openings are provided at the junction of reaction chamber 2 andinjection device 21.

The exemplary injection device of FIG. 20 comprises a slide bar 22, aspike 23, and an injection lance 24. The injection device is adapted forholding one or several constituents of the composition for generatingoxygen, in the illustrated example the ionic liquid 8. Ionic liquid 8 iscontained in a receptacle 5 made from a material which can be easilyruptured, for example a plastic foil. A mixture of peroxide 7 andcatalyst 9 is contained in reaction chamber 2. Alternatively, catalyst 9may be contained in ionic liquid 8. In a device as illustrated in FIG.20, any settlement of the catalyst within the ionic liquid duringstorage does not constitute a disadvantage because the catalyst will bere-dispersed during the injection step.

Slide bar 22 can be actuated in an analogous manner as the breakingdevice 18 in FIG. 18, and the cutting device 20 in FIG. 19. Onceactuated, slide bar 22 pushes receptacle 5 towards spike 23, receptacle5 is ruptured, and ionic liquid 8 is injected through injection lance 24into reaction chamber 2. Preferably, injection lance 24 is provided withseveral holes (not shown) in order to provide uniform distribution ofionic liquid 8. Ionic liquid 8 soaks the mixture of peroxide 7 andcatalyst 9, or alternatively the mixture of ionic liquid 8 and catalyst9 soaks peroxide 7, and the peroxide decomposition reaction starts,generating oxygen. The oxygen leaves reaction chamber 2 via membranes16.

Analogously to the embodiments described above, the arrangement ofperoxide 7, ionic liquid 8, and metal oxide catalyst 9 may be differentfrom the arrangement illustrated in FIG. 20. In particular, if not aliquid, but solid matter is contained in the injection device or dosingunit 21, no receptacle 5 is required, and means for destroying thereceptacle, such as spike 23, and an injection lance are also notrequired.

FIG. 21 depicts an embodiment of the device 1 for generating oxygenwhich is similar to the embodiment depicted in FIG. 18. Different fromthe embodiment of FIG. 18, the device for generating oxygen of FIG. 21is contained in a container 10 surrounding and protecting reactionchamber 2. In this case, the oxygen generated is not directly releasedinto the environment, but rather enters into a gas space 11 between gaspermeable membrane 16 and an upper wall of container 10. The oxygenexits gas space 11 via a gas outlet 12 which may be, for example,provided with a filter.

A device 1 as shown in FIG. 21 typically does not need any furtherthermal insulation. Rather, container 10 provides for sufficientinsulation. If desired, a thin layer (for example, having a thickness ofabout 1 to 3 mm) of an insulating material may be placed between theouter wall of reaction chamber 2 and the inner wall of container 10.Such an insulating material may also serve the additional purpose ofholding reaction chamber 2 tightly fixed in place within container 10.No insulating material should be provided between membrane 16 and thecontainer wall opposite to membrane 16, i.e. in gas space 11.

Housing the reaction chamber within a container is advantageous both indevices for generating oxygen having only one reaction chamber, and indevices for generating oxygen having more than one reaction chamber, forexample two reaction chambers or a plurality or multitude of reactionchambers 2. An embodiment having eight reaction chambers 2 isillustrated in FIG. 22.

In the device for generating oxygen illustrated in FIG. 22, reactionchambers 2 are shown schematically. Generally, the construction ofreaction chambers 2 is not limited in any manner. For example, reactionchambers as illustrated in FIGS. 18 to 20 can be used. Furthermore, thearrangement of the reaction chambers is not limited to the arrangementshown in FIG. 22. Rather, the reaction chambers may be arranged withinthe container 10 in any appropriate manner.

Oxygen generation within reaction chambers 2 is initiated uponactivation of reaction chambers 2. In the embodiment shown in FIG. 22,all reaction chambers 2 are activated simultaneously by a commonactivation mechanism 19, such as a spring, designed for pushing a plate18 towards reaction chambers 2, as described in connection with FIG. 18.Alternatively, each reaction chamber may be activated individually, i.e.may have its own activation mechanism, or several reaction chambers maybe arranged to groups, each group having its own activation mechanism.For example, in the embodiment of FIG. 22, the eight reaction chambersmight be arranged into two groups of four chambers, each group havingits own activation mechanism.

Container 10 provides a gas space 11 receiving oxygen from all reactionchambers 2, and the oxygen collected within gas space 11 exits gas space11 via gas outlet 12. Alternatively, gas space 11 may be divided into aplurality of compartments. A separate compartment, having its own gasoutlet, may be attributed to each reaction chamber 2, or one compartmentmay provide a common gas space for a group of reaction chambers 2. Forexample, container 10 may provide two gas spaces 11, and each gas space11 may collect oxygen from four reaction chambers 2.

A device for generating oxygen having several reaction chambers 2 allowsto extend oxygen generation over a long time span. As explained above,the reaction time of the peroxide decomposition reaction as well as theonset of the decomposition reaction can be manipulated by choosingappropriate metal oxide catalysts, by varying catalyst amounts and, inparticular, by minimizing or maximizing the accessible surface area ofthe peroxide compound, for example by milling the peroxide compound to afine powder or by pressing the peroxide compound into powder compacts.The higher the compacting pressure, the higher the density of theresulting powder compacts will be, thus minimizing the accessiblesurface area of the peroxide compound.

In a device as illustrated in FIG. 22, each of the eight reactionchambers 2 may be charged with a different composition for generatingoxygen. A first chamber may be charged for example, with a compositioncomprising the peroxide compound in fine powdered form, and a highcatalyst concentration. This chamber will generate oxygen immediatelyupon activation, and with a high reaction rate. Thus, breathable oxygenwill be available immediately, but only for a short time span.

Three further reaction chambers 2 may be charged also with peroxidecompound in fine powdered form, and with catalyst concentrationsdecreasing from chamber to chamber. In these reaction chambers oxygengeneration will be slower, thus extending the time span whereinbreathable oxygen is available.

The remaining four reaction chambers may be charged with peroxidecompound which has been pressed into powder compacts, the compactingpressure increasing from chamber to chamber. In these chambers, theonset of the decomposition reaction will be delayed, the delayincreasing with increasing compaction pressure. This measure furtherextends the time span wherein breathable oxygen is available.

A similar result can be achieved with only one reaction chamber 2 bycharging the single reaction chamber with different oxygen generatingcompositions, for example with different metal oxide catalysts and/orwith oxygen sources in powder form and/or compressed with differentcompacting pressures.

Since the decomposition reactions are scalable to different reactorsizes, it is easily possible to charge an oxygen generating device withan oxygen generating composition in a sufficient amount to provide forthe desired oxygen flow rate. For emergency systems it is generallydesired to produce at least 4 1 oxygen per minute.

Of course, also different numbers of reaction chambers than thosedisclosed by way of example can be advantageously used.

The devices for generating oxygen may be designed as disposable devices(single use) filled with a composition for generating oxygen orcompositions for generating oxygen, respectively, or as reusable deviceswhich can be recharged after use with another composition for generatingoxygen. Therefore, the constituents of the compositions for generatingoxygen can be provided in the form of components suitable for recharginga device for generating oxygen, for example in cartridges.

In an exemplary embodiment, one component comprises a metal oxidecompound formulation and an ionic liquid formulation, and anothercomponent comprise an oxygen source formulation.

In another exemplary embodiment one component comprises an oxygen sourceformulation and a metal oxide compound formulation, and anothercomponent comprises an ionic liquid formulation.

In a further exemplary embodiment, one component comprises an oxygensource formulation, another component comprises an ionic liquidformulation, and still another component comprises a metal oxidecompound formulation.

The term “oxygen source formulation” means that the oxygen source may beone single peroxide compound, but may be as well a combination of two ormore peroxide compounds, and may optionally contain any additives notdetrimentally interacting with the peroxide decomposition reaction.

The term “ionic liquid formulation” means that the ionic liquid may beone single ionic liquid, but may be as well a combination of two or moreionic liquids, and may optionally contain any additives notdetrimentally interacting with the peroxide decomposition reaction. Theionic liquids themselves shall not react with any of the constituents ofthe compositions for generating oxygen, or with any intermediateproducts generated during the decomposition reaction.

The term “metal oxide compound formulation” means that the catalyst maybe one single metal oxide compound, but may be as well a combination oftwo or more metal oxide compounds, and may optionally contain anyadditives not detrimentally interacting with the peroxide decompositionreaction.

The devices for generating oxygen according to the present invention arenot sensitive to interruptions of the oxygen production process, incontrast to chlorate candles which can be easily destabilized, forexample by shaking. Shaking a device for generating oxygen according tothe present invention enhances mixing of the constituents of the oxygengenerating composition and, therefore, promotes the oxygen generationreaction.

The inventive devices can be construed in such a manner that theorientation of the inventive devices for generating oxygen in thegravity field of the earth is arbitrary. To this end, several oxygenoutlets (sealed by gas permeable membranes or other structures allowingpassage of oxygen, while blocking passage of non gaseous substances)must be provided in the walls of reaction chamber(s) 2, and the openingsmust be arranged in such a manner, that there is always an opening whichis not covered by ionic liquid, irrespective of the orientation of thedevice.

1. A device for generating oxygen comprising: at least one reactionchamber for housing a composition for generating oxygen, the compositioncomprising a combination of constituents consisting of at least oneoxygen source, at least one ionic liquid, and at least one metal oxidecompound; means for maintaining at least one of the oxygen source, theionic liquid and the metal oxide compound physically separated from theremaining constituents; means for establishing physical contact of theoxygen source, the ionic liquid and the metal oxide compound; and meansfor allowing oxygen to exit the reaction chamber; wherein the metaloxide compound is an oxide of a single metal or of two or more differentmetals, said metal(s) being selected from the metals of groups 2 to 14of the periodic table of the elements, and wherein the oxygen sourcecomprises a peroxide compound.
 2. The device according to claim 1,wherein the means for allowing oxygen to exit the reaction chamber isselected from a gas permeable membrane, a frit and a molecular sieve. 3.The device according to claim 1, wherein the reaction chamber comprisesa first compartment for receiving at least one of the oxygen source, theionic liquid and the metal oxide compound, and a second compact intentfor receiving the other constituents.
 4. The device according to claim1, wherein the means for maintaining at least one of the oxygen source,the ionic liquid and the metal oxide compound physically separatedcomprise at least one receptacle within the chamber for receiving atleast one of the oxygen source, the ionic liquid and the metal oxidecompound.
 5. The device according to claim 1, wherein the means formaintaining at least one of the oxygen source, the ionic liquid and themetal oxide compound physically separated comprise a membrane, a foil,or a glass plate between the first compartment and the secondcompartment.
 6. The device according to claim 1, wherein the means forestablishing physical contact is a syringe or a dosing mechanism, orcomprise a device for destroying the means for maintaining theconstituents physically separated, and an activation mechanism foractivating the device.
 7. The device according to claim 1, wherein thedevice for destroying is a solid plate, a grid, or a cutting edge. 8.The device according to claim 1, wherein the at least one reactionchamber is placed within a container having a gas outlet.
 9. The deviceaccording to claim 1, wherein at least two reaction chambers or at leastfour reaction chambers are placed within a container, the containerproviding a common gas space for receiving oxygen exiting the reactionchambers.
 10. The device according to claim 1, wherein the at least onereaction chamber comprises different compositions for generating oxygen,or wherein at least two reaction chambers comprise differentcompositions for generating oxygen.
 11. The device according to claim 8,wherein the gas outlet comprises means for restricting gas flow.
 12. Thedevice according to claim 10, wherein the compositions for generatingoxygen differ with respect to the oxygen source and/or with respect tothe ionic liquid and/or with respect to the metal oxide compound and/orwith respect to degree of compaction of the oxygen source.
 13. A chargecomponent for a device for generating oxygen as claimed in claim 1, thecharge component comprising: an oxygen source formulation and/or anionic liquid formulation or a metal oxide compound formulation, whereinthe oxygen source formulation comprises a peroxide compound, the ionicliquid formulation is in the liquid state at least in a temperaturerange from −10° C. to +50° C., and the metal oxide compound formulationcomprises an oxide of one single metal or of two or more differentmetals, said metal(s) being selected from the metals of groups 2 to 14of the periodic table of the elements.
 14. The charge componentaccording to claim 13, wherein the ionic liquid formulation comprises anionic liquid having a cation and an anion, wherein the cation isselected from the group consisting of imidazolium, pyrrolidinium,ammonium, choline, pyridinium, pyrazolium, piperidinium, phosphonium,and sulfonium cations, and wherein the cation may have at least onesubstituent, and wherein the anion is selected from the group consistingof dimethylphosphate, methylsulfate, trifluoromethylsulfonate,bis(trifluoromethylsulfonyl)imide, chloride, bromide, iodide,tetrafluoroborate, and hexafluorophosphate.
 15. The charge componentaccording to claim 13, wherein at least one of the oxygen sourceformulation and the metal oxide compound formulation is in the form ofpowders or is in the form of at least one powder compact.
 16. The chargecomponent according to claim 14, wherein at least one of the oxygensource formulation and the metal oxide compound formulation is in theform of powders or is in the form of at least one powder compact.